CN113750966A - Sludge biological adsorption material for defluorination and preparation method thereof - Google Patents
Sludge biological adsorption material for defluorination and preparation method thereof Download PDFInfo
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- CN113750966A CN113750966A CN202111164459.1A CN202111164459A CN113750966A CN 113750966 A CN113750966 A CN 113750966A CN 202111164459 A CN202111164459 A CN 202111164459A CN 113750966 A CN113750966 A CN 113750966A
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/041—Oxides or hydroxides
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
- B01J2220/4887—Residues, wastes, e.g. garbage, municipal or industrial sludges, compost, animal manure; fly-ashes
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/12—Halogens or halogen-containing compounds
- C02F2101/14—Fluorine or fluorine-containing compounds
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- Chemical & Material Sciences (AREA)
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- Environmental & Geological Engineering (AREA)
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- Life Sciences & Earth Sciences (AREA)
- Treatment Of Sludge (AREA)
- Water Treatment By Sorption (AREA)
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Abstract
The application discloses a sludge biological adsorption material for defluorination and a preparation method thereof, wherein dried sludge powder is pyrolyzed for 40-60min at the temperature of 600-650 ℃ to obtain sludge biochar; mixing the sludge biochar with potassium acetate according to the mass ratio of 1:0.5-2, then pyrolyzing for 40-60min at the temperature of 600-650 ℃, centrifuging, washing, drying and crushing to obtain sludge-based biochar; dissolving aluminum chloride and cerium chloride in deionized water to prepare a mixed solution, and fully mixing the mixed solution with the biochar prepared in the step 2; then dropwise adding a sodium hydroxide solution into the mixed solution, adjusting the pH value of the solution to 7-7.5, fully stirring for 10-12 hours, centrifuging, washing, drying and crushing to prepare the sludge biological adsorption material for defluorination; the removal efficiency can reach more than 80 percent when the fluoride is adsorbed, and the adsorption capacity is 80-110 mg/g.
Description
Technical Field
The invention belongs to the technical field of wastewater defluorination, and particularly relates to a sludge biological adsorption material for defluorination and a preparation method thereof.
Background
In recent years, the removal of fluoride from water mainly comprises a precipitation flocculation method, a membrane treatment method, an ion exchange method and an adsorption method. Wherein the precipitation flocculation method has the defects of poor treatment effect and difficult precipitation of generated fine particles; the membrane treatment method has the defects of being not suitable for wastewater containing solid particles with high salinity and complete dissolution, being easily polluted by membranes and having higher cost; the ion exchange method has the defects of higher cost of ion exchange resin, lower pH value of the treated water, higher chloride content sometimes and certain limitation on application and popularization. Only adsorption has proven to be a low cost, easy to operate technique, and the amount of harmless waste produced by adsorption is relatively small compared to other techniques. Adsorption defluorination is considered to be the most promising defluorination treatment method due to the advantages of low material cost, controllable operation conditions, high adsorption capacity, potential for reuse, regeneration possibility and the like.
On the other hand, with the rapid development of our country's economy, the urban sewage yield and discharge amount are increasing day by day, and it is counted that our country's annual sludge yield is over 6000 million tons at present, which causes a huge burden on the environment. The sludge contains a large amount of microorganisms such as bacteria and viruses, heavy metal ions, substances such as difficultly-degraded organic pollutants and the like, so the sludge needs to be subjected to sanitary treatment, otherwise, secondary pollution is caused, and the environment is harmed. Because the work of sludge treatment in China is carried out later, although various technologies are various, the unified standard is not provided, and the main treatment methods of sludge in China mainly comprise sanitary landfill, sludge composting and drying incineration. However, these disposal methods have problems of land resource occupation, odor generation, and transportation cost. Therefore, the problem of sludge disposal and resource utilization has been receiving attention from people in various fields, and has been identified as a "future waste problem".
Chinese patent CN202110672044.9 discloses a multi-effect defluorination medicament and a preparation method and application thereof. The multi-effect defluorination medicament comprises the following components in parts by weight: polyaluminium salts with Al2O33-10 parts of polymeric aluminum ferric salt and Al2O38-15 parts of oxidant, 2-10 parts of acetate, 3-6 parts of poly dimethyl diallyl ammonium chloride, 0.5-1.5 parts of iminodiacetic acid, 1-3 parts of iminodiacetic acid and 2-3 parts of aluminum chlorohydroxide. The defluorination medicament can ensure that the concentration of fluorine ions in the treated water is less than or equal to 10mg, can meet the requirements of surface water III specified in GB3838-2002 surface water environmental quality standard, has the functions of removing fluorine, removing nitrogen, removing phosphorus and removing COD, has stable removal effect, can realize higher removal rate under lower addition amount, has less addition amount, generates less sludge in the treatment process, is easier to treat the sludge and has low comprehensive cost, but has the defects of poor treatment effect, occupation of land resources and generation of odor in the prior art.
Disclosure of Invention
The technical problem to be solved is as follows:
aiming at the defects of the prior art, the method solves the problems that the existing treatment effect is poor, generated fine particles are difficult to precipitate, and are easy to be polluted by a membrane, the cost is high, the pH value of treated water is low, and the chloride content is sometimes high; provides a sludge biological adsorption material for defluorination and a preparation method thereof.
The technical scheme is as follows:
in order to achieve the purpose, the application is realized by the following technical scheme:
a sludge biological adsorption material for defluorination and a preparation method thereof are provided, wherein the preparation method comprises the following specific steps:
step 1: pyrolyzing the dried sludge powder at the temperature of 600-650 ℃ for 40-60min to obtain sludge biochar;
step 2, mixing the sludge biochar with potassium acetate according to the mass ratio of 1:0.5-2, then pyrolyzing the mixture for 40-60min at the temperature of 600-650 ℃, centrifuging, washing, drying and crushing the mixture to obtain sludge-based biochar;
step 3, dissolving aluminum chloride and cerium chloride in deionized water to prepare a mixed solution, and fully mixing the mixed solution with the sludge-based biochar prepared in the step 2;
and 4, dropwise adding a sodium hydroxide solution into the mixed solution, adjusting the pH value of the solution to 7-7.5, fully stirring for 10-12 hours, centrifuging, washing, drying and crushing to obtain the sludge biological adsorption material for defluorination.
As a preferred technical scheme of the invention: the molar ratio of the aluminum chloride to the cerium chloride in the step 3 is 2: 1.
As a preferred technical scheme of the invention: the mass volume ratio of the sludge-based biochar to the mixed liquor in the step 3 is 0.5-1g:50 mL.
As a preferred technical scheme of the invention: before the sludge-based biochar is mixed with the mixed liquid in the step 3, 100 parts of sludge-based biochar, 0-5 parts of graphene, 2-4 parts of peroxy acetamide and 1-3 parts of carbide slag are weighed according to the mass part ratio, ultrasonically dispersed for 2 hours, centrifuged at the speed of 3000rpm, ground after vacuum drying, sieved by a 200-mesh and 400-mesh sieve to treat the sludge-based biochar, and then added into the mixed liquid according to the mass volume ratio of the treated sludge-based biochar to the mixed liquid of 0.5-1g:50 mL.
As a preferred technical scheme of the invention: the concentration of the sodium hydroxide solution in the step 4 is 1-3 mol/L.
As a preferred technical scheme of the invention: the drying temperature in the step 2 and the step 4 is 60-90 ℃.
The application also discloses the sludge biological adsorption material for defluorination prepared by the preparation method.
Has the advantages that:
the application provides a sludge biological adsorption material for defluorination and a preparation method thereof, compared with the prior art, the sludge biological adsorption material has the following beneficial effects:
1. loading aluminum ions and cerium ions on biochar by utilizing the characteristic that fluoride has strong affinity to metal ions to obtain a novel adsorbing material for removing fluoride in wastewater;
2. provides a sludge biological adsorption material for removing fluorine, which is used for bimetal modified sludge-based adsorption for removing fluorine in water.
3. Compared with the prior art, the invention recycles the waste and well converts the sludge into the biochar with larger specific surface area.
4. The removal efficiency can reach more than 80 percent when the fluoride is adsorbed, and the adsorption capacity is 80-110 mg/g.
5. The technology pyrolyzes the sludge into sludge-based biochar with rich pore diameter and large specific surface area by specific temperature and proportion, and loads metal ions with affinity to fluoride ions onto the sludge biochar by an alkali precipitation method.
6. The technology utilizes the waste of the sludge; the operation is simple and convenient; the types and the content of the materials are less.
Detailed Description
The following will further explain the embodiments and working procedures of the present invention by referring to examples.
Example 1:
a sludge biological adsorption material for defluorination and a preparation method thereof are provided, which comprises the following steps:
step 1: pyrolyzing the dried sludge powder at 600 ℃ for 40min to obtain sludge biochar;
step 2, mixing the sludge biochar with potassium acetate according to the mass ratio of 1:0.5, then pyrolyzing the mixture for 40min at 600 ℃, centrifuging, washing, drying and crushing the mixture to obtain sludge-based biochar; the drying temperature is 60 ℃;
step 3, dissolving aluminum chloride and cerium chloride in deionized water to prepare a mixed solution, and fully mixing the mixed solution with the biochar prepared in the step 2; the molar ratio of the aluminum chloride to the cerium chloride is 2: 1; the mass volume ratio of the biochar to the mixed solution is 0.5g:50 mL;
step 4, dropwise adding a sodium hydroxide solution into the mixed solution, adjusting the pH value of the solution to 7, fully stirring for 10 hours, centrifuging, washing, drying and crushing to obtain the sludge biological adsorption material for defluorination; the concentration of the sodium hydroxide solution is 1 mol/L; the drying temperature is 60 ℃.
Example 2:
a sludge biological adsorption material for defluorination and a preparation method thereof are provided, which comprises the following steps:
step 1: pyrolyzing the dried sludge powder at 630 ℃ for 50min to obtain sludge biochar;
step 2, mixing the sludge biochar with potassium acetate according to the mass ratio of 1:1.8, then pyrolyzing the mixture for 50min at 630 ℃, centrifuging, washing, drying and crushing the mixture to obtain sludge-based biochar; the drying temperature is 80 ℃;
step 3, dissolving aluminum chloride and cerium chloride in deionized water to prepare a mixed solution; weighing 100 parts of sludge-based biochar, 5 parts of graphene, 2-4 parts of peroxy acetamide and 1-3 parts of carbide slag according to the mass part ratio, ultrasonically dispersing for 2 hours, centrifuging at the speed of 3000rpm, drying in vacuum, grinding, sieving with a 200-mesh sieve and 400-mesh sieve to treat the sludge-based biochar, and then fully mixing the treated sludge-based biochar with mixed liquor according to the mass-volume ratio of 0.8g to 50mL of the treated sludge-based biochar to the mixed liquor; the molar ratio of the aluminum chloride to the cerium chloride is 2: 1;
step 4, dropwise adding a sodium hydroxide solution into the mixed solution, adjusting the pH value of the solution to 7.2, fully stirring for 11 hours, centrifuging, washing, drying and crushing to obtain the sludge biological adsorption material for defluorination; the concentration of the sodium hydroxide solution is 2 mol/L; the drying temperature is 80 ℃.
Example 3:
a sludge biological adsorption material for defluorination and a preparation method thereof are provided, which comprises the following steps:
step 1: pyrolyzing the dried sludge powder at 650 ℃ for 60min to obtain sludge biochar;
step 2, mixing the sludge biochar with potassium acetate according to the mass ratio of 1: 2, then pyrolyzing the mixture for 60min at 650 ℃, centrifuging, washing, drying and crushing the mixture to obtain sludge-based biochar; the drying temperature is 90 ℃;
step 3, dissolving aluminum chloride and cerium chloride in deionized water to prepare a mixed solution, and fully mixing the mixed solution with the biochar prepared in the step 2; the molar ratio of the aluminum chloride to the cerium chloride is 2: 1; the mass volume ratio of the biochar to the mixed solution is 1g:50 mL;
step 4, dropwise adding a sodium hydroxide solution into the mixed solution, adjusting the pH value of the solution to 7.5, fully stirring for 12 hours, centrifuging, washing, drying and crushing to prepare the sludge biological adsorption material for defluorination; the concentration of the sodium hydroxide solution is 1-3 mol/L; the drying temperature is 90 ℃.
The removal rate of 20mg/L fluoride reaches more than 95%, the adsorption capacity is 100 mg/g, and the water environment adaptive pH range is 4-9.
Finally, the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and other modifications or equivalent substitutions made by the technical solutions of the present invention by the person skilled in the art shall be covered by the scope of the claims of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (7)
1. A preparation method of a sludge biological adsorption material for defluorination is characterized by comprising the following steps: the preparation method comprises the following specific steps:
step 1: pyrolyzing the dried sludge powder at the temperature of 600-650 ℃ for 40-60min to obtain sludge biochar;
step 2, mixing the sludge biochar with potassium acetate according to the mass ratio of 1:0.5-2, then pyrolyzing the mixture for 40-60min at the temperature of 600-650 ℃, centrifuging, washing, drying and crushing the mixture to obtain sludge-based biochar;
step 3, dissolving aluminum chloride and cerium chloride in deionized water to prepare a mixed solution, and fully mixing the mixed solution with the sludge-based biochar prepared in the step 2;
and 4, dropwise adding a sodium hydroxide solution into the mixed solution, adjusting the pH value of the solution to 7-7.5, fully stirring for 10-12 hours, centrifuging, washing, drying and crushing to obtain the sludge biological adsorption material for defluorination.
2. The method for preparing the sludge biosorption material for defluorination according to claim 1, which comprises the steps of: the molar ratio of the aluminum chloride to the cerium chloride in the step 3 is 2: 1.
3. The method for preparing the sludge biosorption material for defluorination according to claim 1, which comprises the steps of: the mass volume ratio of the sludge-based biochar to the mixed liquor in the step 3 is 0.5-1g:50 mL.
4. The method for preparing the sludge biosorption material for defluorination according to claim 3, wherein: before the sludge-based biochar is mixed with the mixed liquid in the step 3, 100 parts of sludge-based biochar, 0-5 parts of graphene, 2-4 parts of peroxy acetamide and 1-3 parts of carbide slag are weighed according to the mass part ratio, ultrasonically dispersed for 2 hours, centrifuged at the speed of 3000rpm, ground after vacuum drying, sieved by a 200-mesh and 400-mesh sieve to treat the sludge-based biochar, and then added into the mixed liquid according to the mass volume ratio of the treated sludge-based biochar to the mixed liquid of 0.5-1g:50 mL.
5. The method for preparing the sludge biosorption material for defluorination according to claim 1, which comprises the steps of: the concentration of the sodium hydroxide solution in the step 4 is 1-3 mol/L.
6. The method for preparing the sludge biosorption material for defluorination according to claim 1, which comprises the steps of: the drying temperature in the step 2 and the step 4 is 60-90 ℃.
7. A sludge biosorption material for defluorination prepared by the preparation method of any one of claims 1 to 6.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114749163A (en) * | 2022-04-18 | 2022-07-15 | 南京大学 | Preparation method of Ce-Al dephosphorization material |
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| CN110947361A (en) * | 2019-11-27 | 2020-04-03 | 南通大学 | Wheat straw biochar adsorbing material for removing fluorine in water and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110947361A (en) * | 2019-11-27 | 2020-04-03 | 南通大学 | Wheat straw biochar adsorbing material for removing fluorine in water and preparation method thereof |
Non-Patent Citations (2)
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| 周树烽等: "KOH改性污泥生物碳及对富营养化水体吸附研究", 《环境科学与技术》 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114749163A (en) * | 2022-04-18 | 2022-07-15 | 南京大学 | Preparation method of Ce-Al dephosphorization material |
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